This study aimed to develop a selective analytical method for the simultaneous determination of seven bisphenol analogues in beverage and canned food samples by using new molecularly imprinted polymer (MIP) as sorbent solid-phase extraction (SPE). Liquid chromatography coupled triple-quadruple tandem mass spectrometry (LC-MS/MS) was used identify quantify target analytes. The MIP-SPE exhibited higher level selectivity purification than traditional SPE method. developed procedures were...

A quantified method for the determination of 17 phthalate esters ( PAE s) in edible vegetable oil by GC ‐ MS with pretreatment acetonitrile extraction and silica/ N ‐( n P ropyl)ethylenediamine‐mixed SPE column was established. By quantification internal standard D 4 d i(2‐ethylhexyl) phthalate, a good linearity range related s observed. The correlation coefficient ranged at 0.994∼1.000, lowest level 0.05∼0.15 mg/L. spiking recoveries were 78.3∼108.9% relative deviations 4.3∼12.1% = 6)....

An isolation method by reversed-phase liquid chromatography coupled with hydrophilic interaction was successfully used to isolate and purify active bufadienolides from Bufo bufo gargarizans Cantor toad skin. In the first step, crude samples were run on an XTerra Prep C18 column. After screening for activity, two fractions chosen further purification. A Click beta-Cyclodextrin (Click-CD) column made in our laboratory second step. Seven compounds, including four stereoisomers, obtained at high...

A gas chromatography coupled with mass spectrometry (GC/MS) method for the simultaneous determination of chlorpromazine and diazepam in pork samples, which are two most often used antipsychotics, has been developed validated. The samples were prepared purified by solid-phase extraction (SPE), then analyzed GC/MS. Chromatography was performed using an HP-5 MS 5% phenyl–95% methylpolysiloxane fused silica capillary column (30 m × 0.25 mm; film thickness μm). had a linear calibration curve over...

By the combination of solid‐phase extraction as well isotope dilution gas chromatography with mass spectrometry, a sensitive and reliable method for determination endocrine‐disrupting chemicals including bisphenol A, 4‐octylphenol, 4‐nonylphenol in vegetable oils was established. The application silica/ N ‐( n ‐propyl)ethylenediamine mixed cartridge achieved relatively low matrix effects oils. Experiments were designed to evaluate derivatization, parameters optimized. estimated limits...

Antiepileptic drugs are the first choice for epilepsy treatment. Monitoring antiepileptic is important to minimize their adverse side effects by choosing optimum drug dosage. An accurate and high throughput supercritical fluid chromatography-tandem mass spectrometry method has been developed simultaneous quantification of several in human plasma. Plasma samples were extracted with ethyl acetate upper organic layer was directly injected into chromatography/mass (SFC-MS/MS) system without...

An integrated online-offline platform was developed combining automated online LC-MS fraction collection, continuous accumulation of selected ions (CASI), and offline top-down electron capture dissociation (ECD) tandem mass spectrometry experiments to identify a low-level, unknown isomeric degradant in formulated drug product during an accelerated stability study. By identifying the diagnostic isoaspartic acid (isoAsp), ECD experiment showed that Asp9 exenatide converted isoAsp9 form...

Abstract Emerging brominated flame retardants (eBFRs) other than polybrominated diphenyl ethers (PBDEs), biphenyls (PBBs) and their derivatives in foods have been focus recent years due to increasing production volumes, indefinite information on toxicities the lack of data occurrence environments, as well humans. In this study, gas chromatography was coupled an atmospheric pressure chemical ionization-tandem mass spectrometry (APGC-MS/MS) for analysis six eBFRs pork, chicken, egg, milk fish....

The Chinese drug pair Danshen (Salvia miltiorrhiza)-Sanqi (Panax ginseng) has been widely used for centuries treating various cardiovascular disorders, among which salvianlic acid B (SAB), ginsenoside Rg1 (GRg1 ), Rb1 (GRb1 ) and notoginsenoside R1 (NGR1 were identified as the major components. present study focused on interaction between these components based investigating their intestinal absorption using Ussing chamber technique. concentrations of SAB, GRg1 , GRb1 NGR1 in perfusate...

We developed a new method, based on alkaline diatomite solid-phase extraction followed by gas chromatography with mass spectrometry, for the simultaneous determination of toxic contaminants ethyl carbamate (EC) and 4-(5-)methylimidazole (4-MEI) in yellow rice wine soy sauce. The optimal conditions were defined. With application extraction, damage to capillary column organic acids was greatly reduced. deuterated EC used as internal standard, linearity calibration curves 4-MEI good correlation...

Mass spectrometry (MS)-based quantitative proteomics has become a critical component of biological and clinical research for identification biomarkers that can be used early detection diseases. In particular, MS-based targeted been recently developed the validation biomarker candidates in complex samples. such approaches, synthetic reference peptides are stable isotope labeled version proteotypic proteins to quantitated as internal standards enabling specific absolute quantification...

A sensitive and rapid analytical method based on alkaline diatomaceous earth extraction followed by GC/MS was developed for the quantitative determination of toxic contaminant ethyl carbamate (EC) in yellow rice wines. The optimal conditions were investigated. With application extraction, damage organic acids to capillary column greatly reduced. By using d5-EC as an internal standard analysis EC, linearity calibration curves good between 10 1000 ng/mL. LOD LOQ 1.7 5.0 μg/kg, respectively....

A method involving cloud point-salting out extraction (CPSOE) coupled with UHPLC-MS/MS was developed for the determination of eleven sulfonamides in milk. In this study, type and concentration surfactant, de-emulsification condition, pH value, volume n-butanol, equilibration temperature time were optimized. For method, linear range SAs from 0.05 to 50 μg L-1, correlation coefficients higher than 0.997. The average recoveries 61.32 91.67%, LOQs less 0.06 kg-1.

Abstract Background Vitamin E deficiencies are prevalent around the world and have become one of major public health issues. It is necessary to determine their levels in human serum for routine clinical practice. Objective In this study, a simple green ionic liquid-based (IL)vortex-assisted (VA) liquid–liquid microextraction (LLME) combined with HPLC was developed simultaneous determination eight vitamin isomers serum. Methods The IL, 1-octyl-methylimidazolium trifluoromethanesulfonate...

A simple, rapid, sensitive and specific method used to screen confirm multi-class diuretics residues in whole bovine milk is described. Thirteen drugs of four different classes including carbonic anhydrase inhibitors, loop, thiazide potassium-sparing were extracted from by acetonitrile followed further purification with hexane. The analytes separated using an ACQUITY UPLC BEH C18 column detected electrospray ionization tandem mass spectrometry (ESI-MS/MS). MS data acquisition was performed a...

Compound-specific stable chlorine isotope analysis (CSIA-Cl) is an important method for identifying sources of organochlorine contaminants and helping assess their quantification transformation processes. However, the present CSIA-Cl challenged by either redundant conversion pretreatment or complicated mathematical correction. To overcome mentioned problems, a novel has been developed eight pesticides using gas chromatography-negative chemical ionization mass spectrometry (GC-NCI-qMS) in...